CN1129922C - For removing radioactive waste liquid137Composite adsorbent for Cs and preparation method thereof - Google Patents
For removing radioactive waste liquid137Composite adsorbent for Cs and preparation method thereof Download PDFInfo
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- CN1129922C CN1129922C CN 01109015 CN01109015A CN1129922C CN 1129922 C CN1129922 C CN 1129922C CN 01109015 CN01109015 CN 01109015 CN 01109015 A CN01109015 A CN 01109015A CN 1129922 C CN1129922 C CN 1129922C
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims description 6
- 239000002901 radioactive waste Substances 0.000 title abstract description 3
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- 229910001410 inorganic ion Inorganic materials 0.000 claims abstract description 12
- 229920002972 Acrylic fiber Polymers 0.000 claims description 19
- 239000010808 liquid waste Substances 0.000 claims description 11
- 230000002285 radioactive effect Effects 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 8
- 229910052793 cadmium Inorganic materials 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 6
- 229910021536 Zeolite Inorganic materials 0.000 claims description 5
- JUWGUJSXVOBPHP-UHFFFAOYSA-B titanium(4+);tetraphosphate Chemical compound [Ti+4].[Ti+4].[Ti+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JUWGUJSXVOBPHP-UHFFFAOYSA-B 0.000 claims description 5
- 239000010457 zeolite Substances 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- YVBOZGOAVJZITM-UHFFFAOYSA-P ammonium phosphomolybdate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])=O.[O-][Mo]([O-])(=O)=O YVBOZGOAVJZITM-UHFFFAOYSA-P 0.000 claims description 4
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003302 ferromagnetic material Substances 0.000 claims description 3
- 239000011964 heteropoly acid Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 2
- 239000004927 clay Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229940113088 dimethylacetamide Drugs 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 239000011572 manganese Substances 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 15
- 230000005307 ferromagnetism Effects 0.000 abstract description 10
- 239000002131 composite material Substances 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 7
- 239000002699 waste material Substances 0.000 abstract description 7
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- 230000005291 magnetic effect Effects 0.000 abstract description 3
- 230000005294 ferromagnetic effect Effects 0.000 abstract 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000007787 solid Substances 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical class CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000009940 knitting Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 210000002268 wool Anatomy 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001661 cadmium Chemical class 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- NRGIRRZWCDKDMV-UHFFFAOYSA-H cadmium(2+);diphosphate Chemical compound [Cd+2].[Cd+2].[Cd+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O NRGIRRZWCDKDMV-UHFFFAOYSA-H 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- -1 compound ion Chemical class 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for removing radioactive waste liquid137Composite adsorbent for Cs and its preparing process, compound adsorbent prepared from Cs and its preparing process137Inorganic ion adsorbent with strong selective adsorption of Cs and ferromagnetic substance Fe3O4The invention makes the inorganic ion adsorbent have ferromagnetism, and can realize solid-liquid separation under the action of an external magnetic field, thereby solving the problem of solid-liquid separation of the adsorbent and the treated waste liquid. The composite adsorbent has good mechanical strength, high temperature resistance, good dynamic performance and good selective adsorption performance, and has practical value of popularization and application.
Description
The invention belongs to radioactive liquid waste processing, disposal field, particularly relate to and removing in the radioactive liquid waste
137Material that Cs adopts and preparation method thereof.
Handle in the radioactive liquid waste now
137The method of Cs has evaporation method, the precipitation method and absorption method etc., and wherein inorganic ions adsorbents adsorb method is used more extensive.Many inorganic ions adsorbents are right
137Cs has good selection adsorbability, as ferrocyanide, heteropolyacid salt, polyvalent metal acid salt, aluminosilicate, hydrous oxid etc.But be the indefiniteness powder mostly, be difficult to realize Separation of Solid and Liquid, the someone utilizes gel method, Method for bonding that this class material is made bead or blocky-shaped particle, the operation of dress post, after these particle post a period of times, particle swelling bonding is blocked, and produces bubble around the particle but waste liquid is flowed through, be difficult to operation, adopt centrifuge method to carry out Separation of Solid and Liquid, apparatus expensive, complicated operation are if adsorbent combines with ferromagnetic material, magnetic method is separated, and Separation of Solid and Liquid is carried out smoothly.
The purpose of this invention is to provide a kind of in the radioactive liquid waste
137Cs has stronger selection adsorbability, has ferromagnetism again, is easy to realize the compound adsorbent of separating from processed waste liquid.For this reason, the present invention also provides the preparation method of this compound adsorbent.
The present invention finishes by implementing following scheme:
A kind ofly be used for removing radioactive liquid waste
137The compound adsorbent of Cs is characterized in that: this compound ion adsorbent is by inorganic ions adsorbent, ferromagnetic material Fe
3O
4Be composited with acrylic fibers, its dry weight amount is than being (1.6～5): (0.25～1.3): (0.24～1.2).Inorganic ions adsorbent wherein can be following one or both: (1) ferrocyanide, as cadmium ferrocyanide, ferrocyanide nickel, copper ferrocyanide etc., (2) heteropolyacid salt such as Lin Molybdenum acid ammonium, phosphomolybdic acid zirconium, phosphotungstate etc., (3) polyvalent metal acid salt is as titanium phosphate, cadmium phosphate etc., (4) aluminum silicate ore, as clay, zeolite etc., (5) aqua oxidation ores is as manganese oxide ore.
The preparation method of compound adsorbent of the present invention finishes by the following technical programs.
Adopt the coated method method for making of acrylic fibers, its step is as follows:
(1) compound concentration is 8.15% acrylic fibers solution, and solvent adopts the DMAC-dimethyl acetamide, heats 60 ℃ to dissolving fully.
(2) selecting granularity for use is above-mentioned inorganic ions adsorbent of 140～180 purposes and Fe
3O
4
(3) press above-mentioned dry weight amount ratio with inorganic ions adsorbent and Fe
3O
4Add in the acrylic fibers solution, stir, then this potpourri is splashed in the deionized water, potpourri solidifies immediately, leaches solidfied material, dries to constant weight under 60 ℃, pulverizes standby.
Compound adsorbent of the present invention is because it is right both to have kept former inorganic material
137The strong adsorbability of Cs, again because of ferromagnetism has been arranged, easy, solved the Separation of Solid and Liquid difficult problem of sorbing material and processed waste water effectively, this compound adsorbent has advantages such as good mechanical property, high temperature resistant and dynamic performance be good, and this method that disposes waste liquid can be applied.
Further illustrate below:
Embodiment 1, cadmium ferrocyanide ferromagnetism compound adsorbent treatment of simulated PWR (presurized water reactor) nuclear power station radioactive liquid waste:
(1) acrylic fibers knitting wool 3.8 restrains and places 42.8 gram dimethyl acetamides, and heat (60 ℃) makes it dissolving a little, after treating all to dissolve, stirs, and preserves under room temperature, and is standby.
(2) get 5 gram cadmium ferrocyanides (140 orders-180 order), 0.6 gram Fe
3O
4Add in the above-mentioned acrylic fibers solution for preparing of 5ml, after stirring, this potpourri is splashed in the deionized water, potpourri solidifies immediately, leaches solidfied material, dries to constant weight under 60 ℃, pulverize standbyly, the composition dry weight amount ratio of this cadmium ferrocyanide ferromagnetism composite inorganic adsorbents is 5/06/0.53.
(3) experimental technique: get the above-mentioned compound adsorbent of 0.05g, 5ml simulation PWR radioactive liquid waste is in the 10ml test tube, and the concussion balance was put test tube neodymium-iron-boron permanent magnet last 5 minute, realized Separation of Solid and Liquid, sample analysis, calculation of distribution coefficient Kd.
(4) experimental result: the compound adsorbent that the present invention proposes, the reaction kinetics performance is good, and reaction velocity is fast, promptly reaches adsorption equilibrium in 20 minutes, and handling with additive method needs a few hours, selects characterization of adsorption good, and Kd reaches 1.4 * 10
4(ml/g), and general Kd is about 1000, i.e. expression has stronger selection adsorbability, and can be used to handle salt content and reach 9% PWR radioactive liquid waste, and conventional method only can be handled the waste liquid of salt content at 2-3%.
Embodiment 2, ammonium phosphomolybdate ferromagnetism compound adsorbent treatments B WR (boiling-water reactor) simulated emission waste liquid:
(1) acrylic fibers knitting wool 3.8 restrains and places 42.8 gram dimethyl acetamides, and heat (60 ℃) makes it dissolving a little, after treating all to dissolve, stirs, and preserves under room temperature, and is standby.
(2) get 5 gram ammonium phosphomolybdates (140 orders-180 order), 0.6 gram Fe
3O
4Add in the above-mentioned acrylic fibers solution for preparing of 5ml, after stirring, this potpourri is splashed in the deionized water, potpourri solidifies immediately, leaches solidfied material, dries to constant weight under 60 ℃, pulverize standbyly, the composition dry weight amount of this ammonium phosphomolybdate ferromagnetism composite inorganic adsorbents is than being ammonium phosphomolybdate/Fe
3O
4/ acrylic fibers=2.5/0.25/0.24.
(3) experimental technique is with embodiment 1.
(4) experimental result: reaction kinetics is functional, can reach balance in 40 minutes, selects excellent adsorption, and Kd reaches 1.4 * 10
3(ml/g), can be used to treatments B WR (boiling-water reactor) radioactive liquid waste.
Embodiment 3, and the actual low radioactive waste liquid of ferromagnetism composite natral mineral powder sorbent treatment China atomic energy institute: the inorganic ions adsorbent adopts natural crystal zeolite, manganese ore.
(1) acrylic fibers knitting wool 3.8 restrains and places 42.8 gram dimethyl acetamides, and heat (60 ℃) makes it dissolving a little, after treating all to dissolve, stirs, and preserves under room temperature, and is standby.
(2) get 5 gram zeolite/MnO
2(140 orders-180 order), 0.6 gram Fe
3O
4Add in the above-mentioned acrylic fibers solution for preparing of 5ml, after stirring, this potpourri is splashed in the deionized water, potpourri solidifies immediately, leaches solidfied material, dries to constant weight under 60 ℃, pulverize standbyly, the composition dry weight amount ratio of this ferromagnetism composite inorganic adsorbents is: zeolite/MnO
2/ Fe
3O
4/ acrylic fibers=1.0/0.6/0.3/0.4.
(3) experimental technique is with embodiment 1.
(4) experimental result: effect is better, Kd=630 ± 24 (ml/g).
Embodiment 4, titanium phosphate sections magnetic compound adsorbent treatment of simulated waste liquid:
(1) acrylic fibers knitting wool 3.8 restrains and places 42.8 gram dimethyl acetamides, and heat (60 ℃) makes it dissolving a little, after treating all to dissolve, stirs, and preserves under room temperature, and is standby.
(2) get 5 gram titanium phosphates (140 orders-180 order), 0.6 gram Fe
3O
4Add in the above-mentioned acrylic fibers solution for preparing of 5ml, after stirring, this potpourri is splashed in the deionized water, potpourri solidifies immediately, leaches solidfied material, dries to constant weight under 60 ℃, pulverize standbyly, the composition dry weight amount of this cadmium ferrocyanide ferromagnetism composite inorganic adsorbents is than being titanium phosphate/Fe
3O
4/ acrylic fibers=5/1.3/1.2.
(3) experimental solutions:
Be added with
137The 0.1M NH of Cs indicator
4NO
3Solution.
(4) experimental technique is with embodiment 1.
(5) experimental result:
Good operation performance, this compound adsorbent is right
137Cs has certain selectivity absorption, because NH
4 +Ion and Cs
+The ion competition, distribution ratio is not very big, Kd=230 ± 10 (ml/g).
Claims (2)
1. one kind is used for removing radioactive liquid waste
137The compound adsorbent of Cs is characterized in that: this compound adsorbent is by inorganic ions adsorbent, ferromagnetic material Fe
3O
4Be composited with acrylic fibers, its dry weight amount is than being (1.6～5): (0.25～1.3): (0.24～1.2), in the component inorganic ions adsorbent can be following in any one or two kinds:
(1) ferrocyanide: cadmium ferrocyanide, copper ferrocyanide, ferrocyanide nickel;
(2) heteropolyacid salt: ammonium phosphomolybdate, phosphomolybdic acid zirconium, phosphotungstate;
(3) polyvalent metal acid salt: titanium phosphate, basic zirconium phosphate;
(4) aluminum silicate ore: zeolite, clay;
(5) aqua oxidation ores: manganese ore;
2. the preparation method of the described compound adsorbent of claim 1, it is characterized in that: compound concentration is 8.15% acrylic fibers solution, and solvent adopts the DMAC-dimethyl acetamide, and heating 60 ℃ all dissolves acrylic fibers; Selecting granularity for use is 140～180 purpose inorganic ions adsorbent and Fe
3O
4With the acrylic fibers solution for preparing, press the dry weight amount than (1.6～5): (0.25～1.3): mix (0.24～1.2), after stirring, splashes in the deionized water and solidify, and leaches solidfied material, dries to constant weight at 60 ℃, pulverizes standby.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01109015 CN1129922C (en) | 2001-02-27 | 2001-02-27 | For removing radioactive waste liquid137Composite adsorbent for Cs and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01109015 CN1129922C (en) | 2001-02-27 | 2001-02-27 | For removing radioactive waste liquid137Composite adsorbent for Cs and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1319849A CN1319849A (en) | 2001-10-31 |
| CN1129922C true CN1129922C (en) | 2003-12-03 |
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Cited By (1)
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| CN101093735B (en) * | 2007-04-11 | 2010-12-15 | 浙江大学 | Adsorbent in use for separating heating element Cs, preparation and application |
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2001
- 2001-02-27 CN CN 01109015 patent/CN1129922C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101093735B (en) * | 2007-04-11 | 2010-12-15 | 浙江大学 | Adsorbent in use for separating heating element Cs, preparation and application |
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|---|---|
| CN1319849A (en) | 2001-10-31 |
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